CN113185281B - Titanium dioxide ceramic material prepared by sol-gel method - Google Patents

Titanium dioxide ceramic material prepared by sol-gel method Download PDF

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CN113185281B
CN113185281B CN202110747833.4A CN202110747833A CN113185281B CN 113185281 B CN113185281 B CN 113185281B CN 202110747833 A CN202110747833 A CN 202110747833A CN 113185281 B CN113185281 B CN 113185281B
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titanium dioxide
ceramic material
magnesium alloy
ion implantation
ions
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CN113185281A (en
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朱剑熹
韩斐
刘俊彦
朱勇
罗浩
郭斌
胡懿郃
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Xiangya Hospital of Central South University
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Xiangya Hospital of Central South University
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Abstract

A titanium dioxide ceramic material prepared by a sol-gel method is prepared by doping rare earth elements cerium and yttrium on the surface of titanium dioxide porous ceramic by an ion implantation method. Essentially, the hole sealing effect can be achieved by ion implantation of rare earth elements, and TiO is formed on the surface or near-surface area of the titanium dioxide ceramic after ion implantation2the-Ce-Y composite ceramic material improves the corrosion resistance of the porous titanium dioxide. It is worth noting that the injection amount of the rare earth element needs to be controlled within a reasonable range, when the injection amount of the rare earth element is too large, a Ce-Y film is formed on the surface of the titanium dioxide ceramic, and when the injection amount of the rare earth element is too small, a proper hole sealing effect cannot be achieved, which is not beneficial to the improvement of the corrosion resistance of the porous titanium dioxide ceramic material.

Description

Titanium dioxide ceramic material prepared by sol-gel method
Technical Field
The invention relates to the field of ceramic materials, in particular to a titanium dioxide ceramic material prepared by a sol-gel method.
Background
In the fields of orthopedics, oral surgery, thoracic surgery and the like, a high-strength material for fracture repair and chest support is required and is called a bone fixing material. The bone fixing material has many kinds, such as needle shape, plate shape, etc., and plays a role in auxiliary connection between bone blocks. At present, the elastic modulus of widely used stainless steel and titanium alloy is far higher than that of human bone, and the stress shielding effect generated by the elastic modulus is not beneficial to the growth and healing of the bone. The elasticity modulus of the magnesium alloy is close to that of human bones, and the stress shielding effect can be effectively relieved. The magnesium alloy can provide stable mechanical property in the early stage of fracture healing, gradually reduce the stress shielding effect, and enable the fracture part to bear stress stimulation which is gradually increased to the physiological level, thereby accelerating the fracture healing and preventing local osteoporosis and recrudescence.
However, magnesium alloys have poor corrosion resistance in human bodies and cannot play a sufficient mechanical supporting role in a corresponding time, so researchers have studied how to improve the corrosion resistance of magnesium alloys for a long time. The surface modification is a widely applied method, and the surface modification of the magnesium alloy comprises a fluoride coating, a rare earth conversion film, a phosphorus conversion coating, a sol-gel coating and the like. Sol-gel coatings are favored because of the low temperature requirements and the ability to operate at ambient temperatures. However, most of the films prepared by the sol-gel method are porous, and the compactness is poor, so that the corrosion resistance of the sol-gel coating can not meet the use requirement under a specific scene.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide the titanium dioxide ceramic material prepared by the sol-gel method, further improve the corrosion resistance of the existing titanium dioxide medical ceramic material, and meet the use requirements of specific medical scenes.
A titanium dioxide ceramic material prepared by a sol-gel method comprises the following steps:
A. selecting magnesium alloy as a substrate material;
B. pretreating the magnesium alloy;
C. preparing a micro-arc oxidation layer;
D. preparing titanium dioxide sol: preparing tetrabutyl titanate precursor solution by taking absolute ethyl alcohol and distilled water as a mixed solvent, wherein the concentration of tetrabutyl titanate is 0.5-0.8mol/L, the volume ratio of the absolute ethyl alcohol to the distilled water is 1-2: 3-5, adding 3-6% of glycerol in the volume of the solution as a thickening agent, and aging for 20-24 h;
E. preparing a titanium dioxide ceramic material: spin-coating the sol obtained in the step D on the surface of the magnesium alloy coated with the micro-arc oxide layer at the spin-coating speed of 2000-2500 rpm, and then drying in an oven at the drying temperature of 180-200 ℃;
F. e, putting the titanium dioxide ceramic material in the step E into a vacuum annealing furnace, and annealing for 2-2.5h at the temperature of 400-450 ℃;
G. ion implantation of rare earth elements: putting the annealed titanium dioxide ceramic material into ion implantation equipment, and adjusting the vacuum degree of the equipment to be not higher than 1 x 10-4Pa, rare earth elements Ce and Y are selected for ion implantation, wherein the ion voltage is 50-80 keV.
Further, the magnesium alloy is a medical magnesium alloy.
Further, the magnesium alloy was cut into a size of 6 × 6 × 2mm in step a.
Further, the pretreatment comprises degreasing, acid washing, cleaning and drying, wherein sodium carbonate solution with the concentration of 10% -15% is selected for degreasing, hydrochloric acid solution with the concentration of 15% -20% is selected for acid washing, the cleaning treatment is absolute ethyl alcohol ultrasonic cleaning, and the drying is carried out in the nitrogen atmosphere.
Further, the step C is to use magnesium alloy as anode in 10-12 A.dm-2Under the conditions of constant current density, pulse frequency of 450-600Hz, duty ratio of 40-45%, and termination voltage of 350-400V, and time of 10-12min, the magnesium alloy micro-arc oxidation layer is prepared, wherein the electrolyte comprises 30-35g/L of sodium hexametaphosphate, 15-20g/L of potassium hydroxide, 8-9g/L of ammonium hydrogen fluoride, 8-12g/L of ammonium dihydrogen phosphate, 15-25ml/L of glycerol, and 60-80ml/L of triethanolamine.
Further, the Ce ion implantation amount is 6 x 1013-6×1015ions/cm2The implantation amount of Y ions is 6X 1013-6×1015ions/cm2。
Preferably, the Ce ion implantation amount is 4 x 1015ions/cm2The implantation amount of Y ions is 4X 1015ions/cm2。
In order to improve the corrosion resistance of the porous titanium dioxide ceramic material prepared by the sol-gel method, the invention further carries out ion implantation treatment on the porous titanium dioxide ceramic material, and rare earth elements of cerium and yttrium are doped on the surface of the porous titanium dioxide ceramic material by the ion implantation method. Essentially, the hole sealing effect can be achieved by ion implantation of rare earth elements, and TiO is formed on the surface or near-surface area of the titanium dioxide ceramic after ion implantation2the-Ce-Y composite ceramic material improves the corrosion resistance of the porous titanium dioxide. It is worth noting that the injection amount of the rare earth element needs to be controlled within a reasonable range, when the injection amount of the rare earth element is too large, a Ce-Y film is formed on the surface of the titanium dioxide ceramic, and when the injection amount of the rare earth element is too small, a proper hole sealing effect cannot be achieved, which is not beneficial to the improvement of the corrosion resistance of the porous titanium dioxide ceramic material.
Detailed Description
The technical effects of the present invention are demonstrated below by specific examples, but the embodiments of the present invention are not limited thereto.
Example 1
The sol-gel method for preparing the titanium dioxide ceramic material comprises the following steps:
A. cutting medical magnesium alloy into 6 × 6 × 2mm size;
B. pretreating the magnesium alloy, wherein the pretreatment comprises degreasing, pickling, cleaning and drying, wherein sodium carbonate solution with the concentration of 10% is selected for degreasing, hydrochloric acid solution with the concentration of 15% is selected for pickling, the cleaning treatment is absolute ethyl alcohol ultrasonic cleaning, and the drying is carried out in a nitrogen atmosphere;
C. preparing a micro-arc oxidation layer: using magnesium alloy as anode at 10 A.dm-2The magnesium alloy micro-arc oxidation layer is prepared under the conditions of constant current density, pulse frequency of 450Hz, duty ratio of 40 percent, end voltage of 400V and time of 10min, wherein the electrolyte comprises 35g/L of sodium hexametaphosphate, 15g/L of potassium hydroxide, 8g/L of ammonium hydrogen fluoride, 12g/L of ammonium dihydrogen phosphate, 25ml/L of glycerol and 80ml/L of triethanolamine.
D. Preparing titanium dioxide sol: preparing tetrabutyl titanate precursor solution by taking absolute ethyl alcohol and distilled water as a mixed solvent, wherein the concentration of tetrabutyl titanate is 0.5mol/L, the volume ratio of absolute ethyl alcohol to distilled water is 1: 3, adding 3% of glycerol in the volume of the solution as a thickening agent, and aging for 24 h.
E. Preparing a titanium dioxide ceramic material: and D, spin-coating the sol obtained in the step D on the surface of the magnesium alloy coated with the micro-arc oxide layer at the spin-coating speed of 2500 rpm, and drying in an oven at the drying temperature of 180 ℃.
F. And E, putting the titanium dioxide ceramic material in the step E into a vacuum annealing furnace, and annealing for 2.5 hours at 400 ℃.
G. Ion implantation of rare earth elements: putting the annealed titanium dioxide ceramic material into ion implantation equipment, and adjusting the vacuum degree of the equipment to 1 x 10-4Pa, rare earth elements Ce and Y are selected for ion implantation, wherein the ion voltage is 80keV, and the Ce ion implantation amount is 6 multiplied by 1015ions/cm2The implantation amount of Y ions is 6X 1015ions/cm2。
Example 2
The sol-gel method for preparing the titanium dioxide ceramic material comprises the following steps:
A. cutting medical magnesium alloy into 6 × 6 × 2mm size;
B. pretreating the magnesium alloy, wherein the pretreatment comprises degreasing, pickling, cleaning and drying, wherein sodium carbonate solution with the concentration of 10% is selected for degreasing, hydrochloric acid solution with the concentration of 15% is selected for pickling, the cleaning treatment is absolute ethyl alcohol ultrasonic cleaning, and the drying is carried out in a nitrogen atmosphere;
C. preparing a micro-arc oxidation layer: using magnesium alloy as anode at 10 A.dm-2The magnesium alloy micro-arc oxidation layer is prepared under the conditions of constant current density, pulse frequency of 450Hz, duty ratio of 40 percent, end voltage of 400V and time of 10min, wherein the electrolyte comprises 35g/L of sodium hexametaphosphate, 15g/L of potassium hydroxide, 8g/L of ammonium hydrogen fluoride, 12g/L of ammonium dihydrogen phosphate, 25ml/L of glycerol and 80ml/L of triethanolamine.
D. Preparing titanium dioxide sol: preparing tetrabutyl titanate precursor solution by taking absolute ethyl alcohol and distilled water as a mixed solvent, wherein the concentration of tetrabutyl titanate is 0.5mol/L, the volume ratio of absolute ethyl alcohol to distilled water is 1: 3, adding 3% of glycerol in the volume of the solution as a thickening agent, and aging for 24 h.
E. Preparing a titanium dioxide ceramic material: and D, spin-coating the sol obtained in the step D on the surface of the magnesium alloy coated with the micro-arc oxide layer at the spin-coating speed of 2500 rpm, and drying in an oven at the drying temperature of 180 ℃.
F. And E, putting the titanium dioxide ceramic material in the step E into a vacuum annealing furnace, and annealing for 2.5 hours at 400 ℃.
G. Ion implantation of rare earth elements: putting the annealed titanium dioxide ceramic material into ion implantation equipment, and adjusting the vacuum degree of the equipment to 1 x 10-4Pa, rare earth elements Ce and Y are selected for ion implantation, wherein the ion voltage is 80keV, and the Ce ion implantation amount is 4 multiplied by 1015ions/cm2The implantation amount of Y ions is 4X 1015ions/cm2。
Example 3
The sol-gel method for preparing the titanium dioxide ceramic material comprises the following steps:
A. cutting medical magnesium alloy into 6 × 6 × 2mm size;
B. pretreating the magnesium alloy, wherein the pretreatment comprises degreasing, pickling, cleaning and drying, wherein sodium carbonate solution with the concentration of 10% is selected for degreasing, hydrochloric acid solution with the concentration of 15% is selected for pickling, the cleaning treatment is absolute ethyl alcohol ultrasonic cleaning, and the drying is carried out in a nitrogen atmosphere;
C. preparing a micro-arc oxidation layer: using magnesium alloy as anode at 10 A.dm-2The magnesium alloy micro-arc oxidation layer is prepared under the conditions of constant current density, pulse frequency of 450Hz, duty ratio of 40 percent, end voltage of 400V and time of 10min, wherein the electrolyte comprises 35g/L of sodium hexametaphosphate, 15g/L of potassium hydroxide, 8g/L of ammonium hydrogen fluoride, 12g/L of ammonium dihydrogen phosphate, 25ml/L of glycerol and 80ml/L of triethanolamine.
D. Preparing titanium dioxide sol: preparing tetrabutyl titanate precursor solution by taking absolute ethyl alcohol and distilled water as a mixed solvent, wherein the concentration of tetrabutyl titanate is 0.5mol/L, the volume ratio of absolute ethyl alcohol to distilled water is 1: 3, adding 3% of glycerol in the volume of the solution as a thickening agent, and aging for 24 h.
E. Preparing a titanium dioxide ceramic material: and D, spin-coating the sol obtained in the step D on the surface of the magnesium alloy coated with the micro-arc oxide layer at the spin-coating speed of 2500 rpm, and drying in an oven at the drying temperature of 180 ℃.
F. And E, putting the titanium dioxide ceramic material in the step E into a vacuum annealing furnace, and annealing for 2.5 hours at 400 ℃.
G. Ion implantation of rare earth elements: putting the annealed titanium dioxide ceramic material into ion implantation equipment, and adjusting the vacuum degree of the equipment to 1 x 10-4Pa, rare earth elements Ce and Y are selected for ion implantation, wherein the ion voltage is 80keV, and the Ce ion implantation amount is 5 multiplied by 1014ions/cm2The implantation amount of Y ions is 5X 1014ions/cm2。
Example 4
The sol-gel method for preparing the titanium dioxide ceramic material comprises the following steps:
A. cutting medical magnesium alloy into 6 × 6 × 2mm size;
B. pretreating the magnesium alloy, wherein the pretreatment comprises degreasing, pickling, cleaning and drying, wherein sodium carbonate solution with the concentration of 10% is selected for degreasing, hydrochloric acid solution with the concentration of 15% is selected for pickling, the cleaning treatment is absolute ethyl alcohol ultrasonic cleaning, and the drying is carried out in a nitrogen atmosphere;
C. preparing a micro-arc oxidation layer: using magnesium alloy as anode at 10 A.dm-2The magnesium alloy micro-arc oxidation layer is prepared under the conditions of constant current density, pulse frequency of 450Hz, duty ratio of 40 percent, end voltage of 400V and time of 10min, wherein the electrolyte comprises 35g/L of sodium hexametaphosphate, 15g/L of potassium hydroxide, 8g/L of ammonium hydrogen fluoride, 12g/L of ammonium dihydrogen phosphate, 25ml/L of glycerol and 80ml/L of triethanolamine.
D. Preparing titanium dioxide sol: preparing tetrabutyl titanate precursor solution by taking absolute ethyl alcohol and distilled water as a mixed solvent, wherein the concentration of tetrabutyl titanate is 0.5mol/L, the volume ratio of absolute ethyl alcohol to distilled water is 1: 3, adding 3% of glycerol in the volume of the solution as a thickening agent, and aging for 24 h.
E. Preparing a titanium dioxide ceramic material: and D, spin-coating the sol obtained in the step D on the surface of the magnesium alloy coated with the micro-arc oxide layer at the spin-coating speed of 2500 rpm, and drying in an oven at the drying temperature of 180 ℃.
F. And E, putting the titanium dioxide ceramic material in the step E into a vacuum annealing furnace, and annealing for 2.5 hours at 400 ℃.
G. Ion implantation of rare earth elements: putting the annealed titanium dioxide ceramic material into ion implantation equipment, and adjusting the vacuum degree of the equipment to 1 x 10-4Pa, rare earth elements Ce and Y are selected for ion implantation, wherein the ion voltage is 80keV, and the Ce ion implantation amount is 6 multiplied by 1013ions/cm2The implantation amount of Y ions is 6X 1013ions/cm2。
Comparative example 1
The sol-gel method for preparing the titanium dioxide ceramic material comprises the following steps:
A. cutting medical magnesium alloy into 6 × 6 × 2mm size;
B. pretreating the magnesium alloy, wherein the pretreatment comprises degreasing, pickling, cleaning and drying, wherein sodium carbonate solution with the concentration of 10% is selected for degreasing, hydrochloric acid solution with the concentration of 15% is selected for pickling, the cleaning treatment is absolute ethyl alcohol ultrasonic cleaning, and the drying is carried out in a nitrogen atmosphere;
C. preparing a micro-arc oxidation layer: using magnesium alloy as anode at 10 A.dm-2The magnesium alloy micro-arc oxidation layer is prepared under the conditions of constant current density, pulse frequency of 450Hz, duty ratio of 40 percent, end voltage of 400V and time of 10min, wherein the electrolyte comprises 35g/L of sodium hexametaphosphate, 15g/L of potassium hydroxide, 8g/L of ammonium hydrogen fluoride, 12g/L of ammonium dihydrogen phosphate, 25ml/L of glycerol and 80ml/L of triethanolamine.
D. Preparing titanium dioxide sol: preparing tetrabutyl titanate precursor solution by taking absolute ethyl alcohol and distilled water as a mixed solvent, wherein the concentration of tetrabutyl titanate is 0.5mol/L, the volume ratio of absolute ethyl alcohol to distilled water is 1: 3, adding 3% of glycerol in the volume of the solution as a thickening agent, and aging for 24 h.
E. Preparing a titanium dioxide ceramic material: and D, spin-coating the sol obtained in the step D on the surface of the magnesium alloy coated with the micro-arc oxide layer at the spin-coating speed of 2500 rpm, and drying in an oven at the drying temperature of 180 ℃.
F. And E, putting the titanium dioxide ceramic material in the step E into a vacuum annealing furnace, and annealing for 2.5 hours at 400 ℃.
G. Ion implantation of rare earth elements: putting the annealed titanium dioxide ceramic material into ion implantation equipment, and adjusting the vacuum degree of the equipment to 1 x 10-4Pa, rare earth elements Ce and Y are selected for ion implantation, wherein the ion voltage is 80keV, and the Ce ion implantation amount is 5 multiplied by 1020ions/cm2The implantation amount of Y ions is 5X 1020ions/cm2。
Comparative example 2
The sol-gel method for preparing the titanium dioxide ceramic material comprises the following steps:
A. cutting medical magnesium alloy into 6 × 6 × 2mm size;
B. pretreating the magnesium alloy, wherein the pretreatment comprises degreasing, pickling, cleaning and drying, wherein sodium carbonate solution with the concentration of 10% is selected for degreasing, hydrochloric acid solution with the concentration of 15% is selected for pickling, the cleaning treatment is absolute ethyl alcohol ultrasonic cleaning, and the drying is carried out in a nitrogen atmosphere;
C. preparing a micro-arc oxidation layer: using magnesium alloy as anode at 10 A.dm-2The magnesium alloy micro-arc oxidation layer is prepared under the conditions of constant current density, pulse frequency of 450Hz, duty ratio of 40 percent, end voltage of 400V and time of 10min, wherein the electrolyte comprises 35g/L of sodium hexametaphosphate, 15g/L of potassium hydroxide, 8g/L of ammonium hydrogen fluoride, 12g/L of ammonium dihydrogen phosphate, 25ml/L of glycerol and 80ml/L of triethanolamine.
D. Preparing titanium dioxide sol: preparing tetrabutyl titanate precursor solution by taking absolute ethyl alcohol and distilled water as a mixed solvent, wherein the concentration of tetrabutyl titanate is 0.5mol/L, the volume ratio of absolute ethyl alcohol to distilled water is 1: 3, adding 3% of glycerol in the volume of the solution as a thickening agent, and aging for 24 h.
E. Preparing a titanium dioxide ceramic material: and D, spin-coating the sol obtained in the step D on the surface of the magnesium alloy coated with the micro-arc oxide layer at the spin-coating speed of 2500 rpm, and drying in an oven at the drying temperature of 180 ℃.
F. And E, putting the titanium dioxide ceramic material in the step E into a vacuum annealing furnace, and annealing for 2.5 hours at 400 ℃.
G. Ion implantation of rare earth elements: putting the annealed titanium dioxide ceramic material into ion implantation equipment, and adjusting the vacuum degree of the equipment to 1 x 10-4Pa, rare earth elements Ce and Y are selected for ion implantation, wherein the ion voltage is 80keV, and the Ce ion implantation amount is 9 multiplied by 1010ions/cm2The implantation amount of Y ions is 9X 1010ions/cm2。
Next, the corrosion resistance of the titania ceramic materials obtained in examples 1 to 4 and comparative examples 1 to 2 was tested, and the titania ceramic material without ion implantation treatment was used as a blank control, specifically: in Simulated Body Fluid (SBF), packaging each experimental sample at 37 ℃ to prevent edge effect, then respectively placing the experimental samples in beakers filled with simulated liquid, sealing the mouths of the beakers by preservative films, placing the beakers in a constant-temperature water bath kettle at 37 ℃, updating the simulated body fluid every two days, and recording the condition that the samples begin to corrode. Table 1 shows the corrosion resistance test data for each sample, wherein "time" indicates the time at which the sample starts to corrode.
TABLE 1 Corrosion resistance test data for each test sample
Figure DEST_PATH_IMAGE002
As can be seen from table 1, after the titanium dioxide porous ceramic material prepared by the sol-gel method is subjected to ion implantation of rare earth elements Ce and Y with appropriate content, the corrosion resistance of the titanium dioxide porous ceramic material can be further improved.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.

Claims (6)

1. The titanium dioxide ceramic material prepared by a sol-gel method is characterized by comprising the following steps:
A. selecting magnesium alloy as a substrate material;
B. pretreating the magnesium alloy;
C. preparing a micro-arc oxidation layer;
D. preparing titanium dioxide sol: preparing tetrabutyl titanate precursor solution by taking absolute ethyl alcohol and distilled water as a mixed solvent, wherein the concentration of tetrabutyl titanate is 0.5-0.8mol/L, the volume ratio of the absolute ethyl alcohol to the distilled water is 1-2: 3-5, adding 3-6% of glycerol in the volume of the solution as a thickening agent, and aging for 20-24 h;
E. preparing a titanium dioxide ceramic material: spin-coating the sol obtained in the step D on the surface of the magnesium alloy coated with the micro-arc oxide layer at the spin-coating speed of 2000-2500 rpm, and then drying in an oven at the drying temperature of 180-200 ℃;
F. e, putting the titanium dioxide ceramic material in the step E into a vacuum annealing furnace, and annealing for 2-2.5h at the temperature of 400-450 ℃;
G. ion implantation of rare earth elements: putting the annealed titanium dioxide ceramic material into ion implantation equipment, and adjusting the vacuum degree of the equipment to be not higher than 1 x 10-4Pa, rare earth elements Ce and Y are selected for ion implantation, wherein the ion voltage is 50-80keV, and the Ce ion implantation amount is 6 x 1013-6×1015ions/cm2The implantation amount of Y ions is 6X 1013-6×1015ions/cm2。
2. The ceramic material of claim 1, wherein: the magnesium alloy is medical magnesium alloy.
3. The ceramic material of claim 1, wherein: in step A, the magnesium alloy is cut into 6X 2mm in size.
4. The ceramic material of claim 1, wherein: the pretreatment comprises degreasing, acid washing, cleaning and drying, wherein sodium carbonate solution with the concentration of 10% -15% is selected for degreasing, hydrochloric acid solution with the concentration of 15% -20% is selected for acid washing, the cleaning treatment is absolute ethyl alcohol ultrasonic cleaning, and the drying is carried out in the nitrogen atmosphere.
5. The ceramic material of claim 1, wherein: the step C is to use magnesium alloy as anode in the range of 10-12 A.dm-2Under the conditions of constant current density, pulse frequency of 450-600Hz, duty ratio of 40-45%, and termination voltage of 350-400V, and time of 10-12min, the magnesium alloy micro-arc oxidation layer is prepared, wherein the electrolyte comprises 30-35g/L of sodium hexametaphosphate, 15-20g/L of potassium hydroxide, 8-9g/L of ammonium hydrogen fluoride, 8-12g/L of ammonium dihydrogen phosphate, 15-25ml/L of glycerol, and 60-80ml/L of triethanolamine.
6. The ceramic material of claim 1, wherein: the Ce ion implantation amount is 4 x 1015ions/cm2The implantation amount of Y ions is 4X 1015ions/cm2。
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